CN105063520A - Annealing treatment on aluminum foil for lithium batteries - Google Patents
Annealing treatment on aluminum foil for lithium batteries Download PDFInfo
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- CN105063520A CN105063520A CN201510417167.2A CN201510417167A CN105063520A CN 105063520 A CN105063520 A CN 105063520A CN 201510417167 A CN201510417167 A CN 201510417167A CN 105063520 A CN105063520 A CN 105063520A
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Abstract
The invention relates to annealing treatment on aluminum foil for lithium batteries and belongs to the technical field of aluminum alloy material processing. The annealing treatment comprises the steps of subjecting lithium battery aluminum foil blank to cold rolling to 4.0mm-5.0 mm, and then performing primary annealing treatment; subjecting the blank after the primary annealing treatment to rough rolling to 0.25mm-0.3 mm, and then performing secondary annealing treatment, wherein the temperature in an annealing furnace during the primary annealing treatment is 585 DEG C-590 DEG C, heating lasts for 15h-20h, and the temperature in the annealing furnace is reduced to 460 DEG C-480 DEG C when the blank surface temperature reaches 460 DEG C-475DEG C, and heat is preserved for 3h-6h; the temperature in the annealing furnace during the secondary annealing treatment is 190 DEG C-220 DEG C, heating lasts for 8h-10h, and the temperature in the annealing furnace is reduced to 195 DEG C-205 DEG C when the blank surface temperature reaches 165 DEG C-170DEG C, and heat is preserved for 6h-8h. By means of the annealing treatment, the two-time annealing treatment is arranged reasonably, component segregation during alloy casting is improved, and an original cast rolling structure is improved, so that products which are uniform in component, uniform in structure and stable in performance are obtained, and the performance of the aluminum foil for the lithium batteries is improved.
Description
Technical field
The present invention relates to a kind of anneal of aluminum foil for lithium battery, belong to the processing technique field of aluminum alloy materials.
Background technology
Along with the raising of people's living standard, the lifting of Environmental awareness, the energy transportation means social demand of clean environmental protection is huge, and electric vehicle has become main traffic instrument in people's life, and the power cell as electrical vehicular power source is lithium cell.The positive electrode electronic collector of lithium cell is aluminium foil.This aluminium foil requires that dimensional precision is high.The corrosion-free Hen ﹑ of aluminium foil surface uniform color, Gan Jing ﹑ is Wu Se Cha ﹑ without defects such as wiping Hua Shang ﹑ unstriateds, and template is smooth, and being generally used for the alloy manufacturing aluminium foil is 1235, and aluminium foil performance is general, makes lithium cell performance general.And in prior art, the Production Flow Chart of producing aluminium foil is: melting-semicontinuous casting-sawing (end to end)-milling face-homogenizing annealing-hot rolling-cold rolling-paper tinsel rolls-shears.Although this preparation method to a certain degree degree can improve compound crushing effect and dislocation distribution, crystal grain thinning is thin, and then improve organization mechanics performance, but still can not meet the lithium cell aluminium foil performance requriements day by day improved constantly, still need the material and the preparation method that study aluminum foil for lithium battery.
Summary of the invention
The present invention is directed to the defect existing for prior art, provide a kind of production cost low, increase substantially the anneal of aluminum foil for lithium battery performance, obtained aluminium foil performance is high.
Above-mentioned purpose of the present invention realizes by following technical proposal: a kind of anneal of aluminum foil for lithium battery, and described anneal comprises the steps:
Aluminum foil for lithium battery blank is first cold-rolled to 4.0-5.0mm, then carries out first time anneal; By the blank coarse rolling after first time anneal to 0.25-0.3mm, then carry out second annealing process;
Wherein, during first time anneal, annealing in-furnace temperature is 585-590 DEG C, and heating 15-20h, when Preform surface temperature reaches 460-475 DEG C, is down to 460-480 DEG C by annealing in-furnace temperature, insulation 3-6h;
In-furnace temperature of annealing during second annealing process is 190-220 DEG C, and heating 8-10h, when Preform surface temperature reaches 165-170 DEG C, is down to 195-205 DEG C by the temperature in annealing furnace, insulation 6-8h.
The present invention improves the component segregation in alloy cast bundle process by the process of increase homogenizing annealing, improve original Microstructure of roll casting to obtain the product of uniform composition, homogeneous microstructure, stable performance, and then improve the performance of aluminum foil for lithium battery.
In the anneal of above-mentioned aluminum foil for lithium battery, aluminum foil for lithium battery heating is smelted into aluminium alloy melt by aluminum foil for lithium battery blank before cold rolling; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment; Again the aluminium alloy melt continuous casting and rolling after filtration is become the aluminum foil for lithium battery blank of 6.0-8.0mm.
Wherein, described refining is skimmed and is specially: after aluminium alloy melt is left standstill 12-18min, carry out repeatedly refining treatment again, the time of refining treatment first time is 18-22min, after refining treatment, (namely from second time refining treatment) refining time is 20-25min for the first time, is spaced apart 2h-3h.
Need add Al-5Ti-B grain-refining agent during described grain refining process, add-on is 1.5-2kg/ ton aluminium alloy.
Described degasification slagging-off in degasification tank, passes into high pure nitrogen carry out degasification to aluminium alloy melt, adjustment graphite rotator rotating speed, ensure the hydrogen content≤0.12ml/100gAl of aluminium liquid, hydrogen content≤0.12ml/100gAl, wherein, nitrogen gas purity requires more than 99.995%, and nitrogen pressure is 0.4-0.5Mpa, the temperature of degasification tank melt is 720-730 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour.
Described filtration is that filtering accuracy is 50 orders and 60 orders with two channels bipolar filter plate slagging-off.
The casting of liquid aluminium alloy melt for stream, by casting and rolling machine Casting Roller, is become blank specifically by case lip before casting and rolling machine by described continuous casting and rolling in roll casting zone.Wherein, front case melt temperature 690-700 DEG C, roll gap 4.6-4.8mm, roll 55-60mm during continuous casting and rolling process, lip opening degree 11-12mm, preload force 180-260T, coiling tension: 40-60kn.Roll casting speed 950-980mm/min, cooler-water temperature 32-38 DEG C.
Can be reached by the quality of cast-rolling stock after continuous casting and rolling process of the present invention: with plate difference≤0.05mm, convexity 0.01-0.05mm, grain fineness number 1 grade, longitudinal tolerance≤0.1mm.Technique raw edges≤2mm, there is not striped and the segregation of impact use in Casting Rolled Sheet coarse micro-grain sample surface.Clearly must wipe roller system before the rolling, and rinse by ROLLING OIL, ROLLING OIL is up-to-standard, and roll dressing is up-to-standard, ensures cold burden rolling simultaneously.Correctly select roll speed, tension force by AGC, AFC template automatic control technology controls template thus obtains excellent template.
When blank is cold rolling, casting and rolling machine gloss level of roll is Ra0.5 μm.
In the anneal of above-mentioned aluminum foil for lithium battery, the aluminium foil finish rolling after second annealing process becomes after cold rolling thickness to be the aluminum foil coil of 0.01-0.05mm by aluminum foil for lithium battery blank, aluminum foil coil is cut to obtain finished product aluminum foil for lithium battery.
Select tension force/speed rolling mode during described aluminum foil coil finish rolling, ACG master mode, F strain is 35-50N/mm
2, backward pull is 35-40N/mm
2, roll speed is 500-700m/min, and rolling load is 250-350T, and oil temperature is 50-55 DEG C, and oil pressure is 3.0-4.0bar, and flow is 50-65%, and roll crown is 0.06mm, gloss level of roll Ra0.12-0.2 μm, and rolling oil additives is 6-8%.
Described cutting is divided by double sheet (or individual) the large volume of aluminium foil to be cut to producing individual aluminum foil coil required.
In the anneal of above-mentioned aluminum foil for lithium battery, composition and the mass percent thereof of described aluminum foil for lithium battery blank are: Fe:0.38-0.45%; Si:0.1-0.15%; Cu:0.03-0.06%; Ti:0.015-0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
As preferably, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.38-0.42%; Si:0.12-0.15%; Cu:0.04-0.06%; Ti:0.018-0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Further preferably, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.39%; Si:0.12%; Cu:0.04%; Ti:0.016%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity, wherein, and Mn+Mg+Zn≤0.03%.
Further preferably, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.40%; Si:0.13%; Cu:0.05%; Ti:0.018%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Further preferably, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.38%; Si:0.15%; Cu:0.04%; Ti:0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Further preferably, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.42%; Si:0.12%; Cu:0.06%; Ti:0.019%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Compared with prior art, tool of the present invention has the following advantages:
1, compared with hot rolling technology of the prior art, the present invention improves the component segregation in alloy cast bundle process by second annealing process, improve original Microstructure of roll casting to obtain the product of uniform composition, homogeneous microstructure, stable performance, be conducive to eliminating the work hardening in cold-rolled process simultaneously, and then improve the performance of aluminum foil for lithium battery.
2, the continuous casting and rolling technical process of the present invention's employing is few, and facility investment is little, and floor space is little, and energy-conserving and environment-protective are good, and production cost is low, and aluminum foil for lithium battery clean surface is without Residual oil.
3, the present invention is by the composition of adjustment aluminium alloy, adds Cu element, by changing the synergy between element, improves the performance of aluminium foil, makes it meet the requirement preparing lithium cell aluminium foil.
4, the aluminum foil for lithium battery mechanical property that obtains of the present invention is better: a: thick difference ± 3%; B: tensile strength 160-190MPa; C: unit elongation>=1.5%; D: pinhole number: 0/m
2; E: moistened surface tension force:>=32 dyne; F: aluminium foil uncoiling performance is good, adhesiveness is excellent.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Embodiment 1
Batching: the composition of adjustment aluminum foil for lithium battery and mass percent: Fe:0.39% thereof; Si:0.12%; Cu:0.04%; Ti:0.016%; Surplus is Al and inevitable impurity, wherein, and Mn+Mg+Zn≤0.03%.
Melting, casting-rolling technology: above-mentioned aluminum foil for lithium battery heating is smelted into aluminium alloy melt; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment, then the aluminium alloy melt continuous casting and rolling after filtering is become the blank of 7.0mm.Wherein, refining is skimmed, grain refining, degasification slagging-off, filtration treatment, continuous casting and rolling be specific as follows:
A, refining are skimmed: gone to by aluminium alloy melt in standing furnace and leave standstill 15min, the temperature of standing furnace is 745 DEG C, then repeatedly refining treatment is carried out, the time of nitrogen refining treatment first time is 20min, surface scum is taken off after refining is complete, after refining treatment, (namely from second time refining treatment) refining time is 22min for the first time, is spaced apart 2.5h;
B, grain refining: aluminium Ti, B grain graining agent is joined degasification tank aluminium liquid ingress by titanium silk feeding machine, the add-on of grain-refining agent is 2.5kg/ ton aluminium alloy melt, carries out modifying-refining to melt;
C, degasification slagging-off: in degasification tank, pass into high pure nitrogen degasification is carried out to aluminium alloy melt, adjustment graphite rotator rotating speed, ensures the hydrogen content≤0.12ml/100gAl of aluminium liquid; For controlling hydrogen content≤0.12ml/100gAl, nitrogen gas purity requires to reach more than 99.995%, and nitrogen pressure is at 0.45Mpa, and the temperature of degasification tank melt is 725 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour;
D, filtration treatment: with the bipolar filter plate slagging-off of two channels, filtering accuracy is 50 orders;
E, continuous casting and rolling: by case lip before casting and rolling machine for stream, by casting and rolling machine Casting Roller, become thickness to be the blank of 7.0mm in roll casting zone by the casting of liquid aluminium alloy melt; Wherein, front case melt temperature 695 DEG C, main frame speed 1100m/min, roll gap 4.7mm, roll 58mm, lip opening degree 11mm, preload force 220T, coiling tension: 50kn, roll casting speed 960mm/min, cooler-water temperature 35 DEG C.
Cold-rolling process: blank is first cold-rolled to 4.8mm, then carry out first time anneal: during first time anneal, annealing in-furnace temperature is 585 DEG C, and heating 18h, when Preform surface temperature reaches 465 DEG C, is down to 470 DEG C by annealing in-furnace temperature, insulation 4h; By the blank coarse rolling after first time anneal to 0.28mm, then carry out second annealing process: in-furnace temperature of annealing during second annealing process is 200 DEG C, heating 9h, when Preform surface temperature reaches 168 DEG C, temperature in annealing furnace is down to 200 DEG C, insulation 6-8h; The aluminum foil coil that thickness is 0.032mm will be rolled in blank after second annealing process.
Paper tinsel pressure process: be that the aluminum foil coil pairing of 0.032mm becomes double sheet thickness to be the pairing aluminum foil coil of 0.064mm by single thickness, in pairing oil, additive level is 0.69%, then be that the pairing aluminum foil coil finish rolling of 0.064mm becomes thickness to be the pairing aluminum foil coil of 0.03mm by two total thickness, finally aluminum foil coil is cut into single thickness be 0.015mm finished product aluminum foil for lithium battery; Wherein, tension force/speed rolling mode is selected during finish rolling, ACG master mode, F strain 45N/mm
2, backward pull 38N/mm
2, roll speed 600m/min, rolling load 300T, oil temperature 52 DEG C, oil pressure 3.5bar, flow 60%, roll crown 0.06mm, gloss level of roll Ra0.16 μm, rolling oil additives 7%; Cut rear F strain 45N/mm
2, backward pull 35N/mm
2, speed 400m/min.
The aluminum foil for lithium battery obtained in the present embodiment is carried out performance test, and result actual (real) thickness is 0.0148mm, and tensile strength is 175N/mm
2, unit elongation is 2%, pinhole number 0/m
2, opening a book property naturally droops < 1.0m, dyne value 33.
Embodiment 2
Batching: the composition of adjustment aluminum foil for lithium battery and mass percent: Fe:0.40% thereof; Si:0.13%; Cu:0.05%; Ti:0.018%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Melting, casting-rolling technology: above-mentioned aluminum foil for lithium battery heating is smelted into aluminium alloy melt; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment, then the aluminium alloy melt continuous casting and rolling after filtering is become the blank of 7.0mm.Wherein, refining is skimmed, grain refining, degasification slagging-off, filtration treatment, continuous casting and rolling be specific as follows:
A, refining are skimmed: gone to by aluminium alloy melt in standing furnace and leave standstill 12min, the temperature of standing furnace is 750 DEG C, then repeatedly refining treatment is carried out, the time of nitrogen refining treatment first time is 18min, surface scum is taken off after refining is complete, after refining treatment, (namely from second time refining treatment) refining time is 25min for the first time, is spaced apart 2h;
B, grain refining: aluminium Ti, B grain graining agent is joined degasification tank aluminium liquid ingress by titanium silk feeding machine, the add-on of grain-refining agent is 3kg/ ton aluminium alloy melt, carries out modifying-refining to melt;
C, degasification slagging-off: in degasification tank, pass into high pure nitrogen degasification is carried out to aluminium alloy melt, adjustment graphite rotator rotating speed, ensures the hydrogen content≤0.12ml/100gAl of aluminium liquid; For controlling hydrogen content≤0.12ml/100gAl, nitrogen gas purity requires to reach more than 99.995%, and nitrogen pressure is at 0.4Mpa, and the temperature of degasification tank melt is 730 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour;
D, filtration treatment: with the bipolar filter plate slagging-off of two channels, filtering accuracy is 60 orders;
E, continuous casting and rolling: by case lip before casting and rolling machine for stream, by casting and rolling machine Casting Roller, become thickness to be the blank of 7.0mm in roll casting zone by the casting of liquid aluminium alloy melt; Wherein, front case melt temperature 690 DEG C, main frame speed 1200m/min, roll gap 4.6mm, roll 60mm, lip opening degree 11mm, preload force 260T, coiling tension: 40kn, roll casting speed 980mm/min, cooler-water temperature 32 DEG C.
Cold-rolling process: blank is first cold-rolled to 4.8mm, then carry out first time anneal: during first time anneal, annealing in-furnace temperature is 590 DEG C, and heating 15h, when Preform surface temperature reaches 475 DEG C, is down to 460 DEG C by annealing in-furnace temperature, insulation 6h; By the blank coarse rolling after first time anneal to 0.25mm, then carry out second annealing process: in-furnace temperature of annealing during second annealing process is 220 DEG C, heating 8h, when Preform surface temperature reaches 170 DEG C, is down to 195 DEG C by the temperature in annealing furnace, insulation 8h; The aluminum foil coil that thickness is 0.03mm will be rolled in blank after second annealing process.
Paper tinsel pressure process: be that the aluminum foil coil pairing of 0.03mm becomes double sheet thickness to be the pairing aluminum foil coil of 0.06mm by single thickness, in pairing oil, additive level is 0.69%, then be that the pairing aluminum foil coil finish rolling of 0.06mm becomes thickness to be the pairing aluminum foil coil of 0.03mm by two total thickness, finally aluminum foil coil is cut into single thickness be 0.015mm finished product aluminum foil for lithium battery; Wherein, tension force/speed rolling mode is selected during finish rolling, ACG master mode, F strain 35N/mm
2, backward pull 40N/mm
2, roll speed 500m/min, rolling load 350T, oil temperature 50 DEG C, oil pressure 4.0bar, flow 50%, roll crown 0.06mm, gloss level of roll Ra0.2 μm, rolling oil additives 6-8%; Cut rear F strain 35N/mm
2, backward pull 40N/mm
2, speed 300m/min.
The aluminum foil for lithium battery obtained in the present embodiment is carried out performance test, and result actual (real) thickness is 0.0151mm, and tensile strength is 176N/mm
2, unit elongation is 2%, pinhole number 0/m
2, opening a book property naturally droops < 1.0m, dyne value 34.
Embodiment 3
Batching: the composition of adjustment aluminum foil for lithium battery and mass percent: Fe:0.38% thereof; Si:0.15%; Cu:0.04%; Ti:0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Melting, casting-rolling technology: above-mentioned aluminum foil for lithium battery heating is smelted into aluminium alloy melt; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment, then the aluminium alloy melt continuous casting and rolling after filtering is become the blank of 7.0mm.Wherein, refining is skimmed, grain refining, degasification slagging-off, filtration treatment, continuous casting and rolling be specific as follows:
A, refining are skimmed: gone to by aluminium alloy melt in standing furnace and leave standstill 18min, the temperature of standing furnace is 740 DEG C, then repeatedly refining treatment is carried out, the time of nitrogen refining treatment first time is 22min, surface scum is taken off after refining is complete, after refining treatment, (namely from second time refining treatment) refining time is 20min for the first time, is spaced apart 3h;
B, grain refining: aluminium Ti, B grain graining agent is joined degasification tank aluminium liquid ingress by titanium silk feeding machine, the add-on of grain-refining agent is 2kg/ ton aluminium alloy melt, carries out modifying-refining to melt;
C, degasification slagging-off: in degasification tank, pass into high pure nitrogen degasification is carried out to aluminium alloy melt, adjustment graphite rotator rotating speed, ensures the hydrogen content≤0.12ml/100gAl of aluminium liquid; For controlling hydrogen content≤0.12ml/100gAl, nitrogen gas purity requires to reach more than 99.995%, and nitrogen pressure is at 0.5Mpa, and the temperature of degasification tank melt is 720 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour;
D, filtration treatment: with the bipolar filter plate slagging-off of two channels, filtering accuracy is 60 orders;
E, continuous casting and rolling: by case lip before casting and rolling machine for stream, by casting and rolling machine Casting Roller, become thickness to be the blank of 7.0mm in roll casting zone by the casting of liquid aluminium alloy melt; Wherein, front case melt temperature 700 DEG C, main frame speed 1000m/min, roll gap 4.8mm, roll 55mm, lip opening degree 12mm, preload force 180T, coiling tension: 60kn, roll casting speed 950mm/min, cooler-water temperature 38 DEG C.
Cold-rolling process: blank is first cold-rolled to 4.8mm, then carry out first time anneal: during first time anneal, annealing in-furnace temperature is 585 DEG C, and heating 20h, when Preform surface temperature reaches 460 DEG C, is down to 480 DEG C by annealing in-furnace temperature, insulation 3h; By the blank coarse rolling after first time anneal to 0.3mm, then carry out second annealing process: in-furnace temperature of annealing during second annealing process is 190 DEG C, heating 10h, when Preform surface temperature reaches 165 DEG C, is down to 205 DEG C by the temperature in annealing furnace, insulation 6h; The aluminum foil coil that thickness is 0.035mm will be rolled in blank after second annealing process.
Paper tinsel pressure process: be that the aluminum foil coil pairing of 0.032mm becomes double sheet thickness to be the pairing aluminum foil coil of 0.064mm by single thickness, in pairing oil, additive level is 0.69%, then be that the pairing aluminum foil coil finish rolling of 0.064mm becomes thickness to be the pairing aluminum foil coil of 0.031mm by two total thickness, finally aluminum foil coil is cut into single thickness be 0.0155mm finished product aluminum foil for lithium battery; Wherein, tension force/speed rolling mode is selected during finish rolling, ACG master mode, F strain 50N/mm
2, backward pull 35N/mm
2, roll speed 700m/min, rolling load 250T, oil temperature 55 DEG C, oil pressure 3.0bar, flow 65%, roll crown 0.06mm, gloss level of roll Ra0.12 μm, rolling oil additives 8%; Cut rear F strain 35N/mm
2, backward pull 40N/mm
2, speed 300m/min.
The aluminum foil for lithium battery obtained in the present embodiment is carried out performance test, and result actual (real) thickness is 0.0152mm, and tensile strength is 173N/mm
2, unit elongation is 2.2%, pinhole number 0/m
2, opening a book property naturally droops < 1.0m, dyne value 34.
Embodiment 4
Batching: the composition of adjustment aluminum foil for lithium battery and mass percent: Fe:0.4% thereof; Si:0.13%; Cu:0.05%; Ti:0.017%; Surplus is Al and inevitable impurity, wherein, and Mn+Mg+Zn≤0.03%.
Melting, casting-rolling technology: above-mentioned aluminum foil for lithium battery heating is smelted into aluminium alloy melt; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment, then the aluminium alloy melt continuous casting and rolling after filtering is become the blank of 7.0mm.Wherein, refining is skimmed, grain refining, degasification slagging-off, filtration treatment, continuous casting and rolling be specific as follows:
A, refining are skimmed: gone to by aluminium alloy melt in standing furnace and leave standstill 15min, the temperature of standing furnace is 746 DEG C, then repeatedly refining treatment is carried out, the time of nitrogen refining treatment first time is 20min, surface scum is taken off after refining is complete, after refining treatment, (namely from second time refining treatment) refining time is 23min for the first time, is spaced apart 2.5h;
B, grain refining: aluminium Ti, B grain graining agent is joined degasification tank aluminium liquid ingress by titanium silk feeding machine, the add-on of grain-refining agent is 2.6kg/ ton aluminium alloy melt, carries out modifying-refining to melt;
C, degasification slagging-off: in degasification tank, pass into high pure nitrogen degasification is carried out to aluminium alloy melt, adjustment graphite rotator rotating speed, ensures the hydrogen content≤0.12ml/100gAl of aluminium liquid; For controlling hydrogen content≤0.12ml/100gAl, nitrogen gas purity requires to reach more than 99.995%, and nitrogen pressure is at 0.43Mpa, and the temperature of degasification tank melt is 722 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour;
D, filtration treatment: with the bipolar filter plate slagging-off of two channels, filtering accuracy is 50 orders;
E, continuous casting and rolling: by case lip before casting and rolling machine for stream, by casting and rolling machine Casting Roller, become thickness to be the blank of 7.0mm in roll casting zone by the casting of liquid aluminium alloy melt; Wherein, front case melt temperature 698 DEG C, main frame speed 1080m/min, roll gap 4.7mm, roll 52mm, lip opening degree 12mm, preload force 200T, coiling tension: 52kn, roll casting speed 970mm/min, cooler-water temperature 36 DEG C.
Cold-rolling process: blank is first cold-rolled to 4.8mm, then carry out first time anneal: during first time anneal, annealing in-furnace temperature is 590 DEG C, and heating 16h, when Preform surface temperature reaches 468 DEG C, is down to 465 DEG C by annealing in-furnace temperature, insulation 5h; By the blank coarse rolling after first time anneal to 0.28mm, then carry out second annealing process: in-furnace temperature of annealing during second annealing process is 210 DEG C, heating 9h, when Preform surface temperature reaches 168 DEG C, is down to 200 DEG C by the temperature in annealing furnace, insulation 7h.
Paper tinsel pressure process: the blank finish rolling after second annealing process become thickness to be the aluminum foil coil of 0.03mm, aluminum foil coil is cut to obtain finished product aluminum foil for lithium battery.Tension force/speed rolling mode is selected, AGC master mode, F strain 42N/mm during finish rolling
2, backward pull 38N/mm
2, roll speed 600m/min, rolling load 300T, oil temperature 52 DEG C, oil pressure 3.6bar, flow 58%, roll crown 0.06mm, gloss level of roll Ra0.18 μm, rolling oil additives 6.5%; Cut rear F strain 45N/mm
2, backward pull 38N/mm
2, speed 460m/min.
The aluminum foil for lithium battery obtained in the present embodiment is carried out performance test, and result actual (real) thickness is 0.031mm, and tensile strength is 180N/mm
2, unit elongation is 2.5%, pinhole number 0/m
2, opening a book property naturally droops < 1.0m, dyne value 34.
Embodiment 5
Batching: the composition of adjustment aluminum foil for lithium battery and mass percent: Fe:0.42% thereof; Si:0.12%; Cu:0.06%; Ti:0.019%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
Melting, casting-rolling technology: above-mentioned aluminum foil for lithium battery heating is smelted into aluminium alloy melt; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment, then the aluminium alloy melt continuous casting and rolling after filtering is become the blank of 7.0mm.Wherein, refining is skimmed, grain refining, degasification slagging-off, filtration treatment, continuous casting and rolling be specific as follows:
A, refining are skimmed: gone to by aluminium alloy melt in standing furnace and leave standstill 12min, the temperature of standing furnace is 750 DEG C, then repeatedly refining treatment is carried out, the time of nitrogen refining treatment first time is 18min, surface scum is taken off after refining is complete, after refining treatment, (namely from second time refining treatment) refining time is 25min for the first time, is spaced apart 2h;
B, grain refining: aluminium Ti, B grain graining agent is joined degasification tank aluminium liquid ingress by titanium silk feeding machine, the add-on of grain-refining agent is 3kg/ ton aluminium alloy melt, carries out modifying-refining to melt;
C, degasification slagging-off: in degasification tank, pass into high pure nitrogen degasification is carried out to aluminium alloy melt, adjustment graphite rotator rotating speed, ensures the hydrogen content≤0.12ml/100gAl of aluminium liquid; For controlling hydrogen content≤0.12ml/100gAl, nitrogen gas purity requires to reach more than 99.995%, and nitrogen pressure is at 0.4Mpa, and the temperature of degasification tank melt is 730 DEG C, and is taken off by the scum silica frost floating up to bath surface with nitrogen bubble in degasification tank every 1 hour;
D, filtration treatment: with the bipolar filter plate slagging-off of two channels, filtering accuracy is 50 orders;
E, continuous casting and rolling: by case lip before casting and rolling machine for stream, by casting and rolling machine Casting Roller, become thickness to be the blank of 7.0mm in roll casting zone by the casting of liquid aluminium alloy melt; Wherein, front case melt temperature 690 DEG C, main frame speed 1200m/min, roll gap 4.6mm, roll 60mm, lip opening degree 11mm, preload force 260T, coiling tension: 40kn, roll casting speed 980mm/min, cooler-water temperature 32 DEG C.
Cold-rolling process: blank is first cold-rolled to 4.8mm, then carry out first time anneal: during first time anneal, annealing in-furnace temperature is 590 DEG C, and heating 15h, when Preform surface temperature reaches 475 DEG C, is down to 460 DEG C by annealing in-furnace temperature, insulation 6h; By the blank coarse rolling after first time anneal to 0.25mm, then carry out second annealing process: in-furnace temperature of annealing during second annealing process is 220 DEG C, heating 8h, when Preform surface temperature reaches 170 DEG C, is down to 195 DEG C by the temperature in annealing furnace, insulation 8h.
Paper tinsel pressure process: the blank finish rolling after second annealing process become thickness to be the aluminum foil coil of 0.03mm, aluminum foil coil is cut to obtain finished product aluminum foil for lithium battery.Tension force/speed rolling mode is selected, AGC master mode, F strain 35N/mm during finish rolling
2, backward pull 40N/mm
2, roll speed 500m/min, rolling load 350T, oil temperature 50 DEG C, oil pressure 3.0bar, flow 65%, roll crown 0.06mm, gloss level of roll Ra0.2 μm, rolling oil additives 6.5%; Cut rear F strain 50N/mm
2, backward pull 40N/mm
2, speed 400m/min.
The aluminum foil for lithium battery obtained in the present embodiment is carried out performance test, and result actual (real) thickness is 0.03mm, and tensile strength is 173N/mm
2, unit elongation is 2.2%, pinhole number 0/m
2, opening a book property naturally droops < 1.0m, dyne value 33.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Although made a detailed description the present invention and quoted some specific embodiments as proof, to those skilled in the art, only otherwise it is obvious for leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (10)
1. an anneal for aluminum foil for lithium battery, is characterized in that, described anneal comprises the steps:
Aluminum foil for lithium battery blank is first cold-rolled to 4.0-5.0mm, then carries out first time anneal; By the blank coarse rolling after first time anneal to 0.25-0.3mm, then carry out second annealing process;
Wherein, during first time anneal, annealing in-furnace temperature is 585-590 DEG C, and heating 15-20h, when Preform surface temperature reaches 460-475 DEG C, is down to 460-480 DEG C by annealing in-furnace temperature, insulation 3-6h;
In-furnace temperature of annealing during second annealing process is 190-220 DEG C, and heating 8-10h, when Preform surface temperature reaches 165-170 DEG C, is down to 195-205 DEG C by the temperature in annealing furnace, insulation 6-8h.
2. the anneal of aluminum foil for lithium battery according to claim 1, is characterized in that, aluminum foil for lithium battery heating is smelted into aluminium alloy melt by aluminum foil for lithium battery blank before cold rolling; Then carry out that refining is skimmed successively, grain refining, degasification slagging-off, filtration treatment; Again the aluminium alloy melt continuous casting and rolling after filtration is become the aluminum foil for lithium battery blank of 6.0-8.0mm.
3. the anneal of aluminum foil for lithium battery according to claim 2, it is characterized in that, described refining is skimmed and is specially: aluminium alloy melt is first left standstill 12-18min, then repeatedly refining treatment is carried out, the time of refining treatment first time is 18-22min, the refining time of second time refining treatment and later refining treatment is 20-25min, is spaced apart 2h-3h.
4. the anneal of aluminum foil for lithium battery according to claim 2, it is characterized in that, degasification is except the hydrogen content≤0.12ml/100gAl of aluminium liquid during Slag treatment, hydrogen content≤0.12ml/100gAl, nitrogen gas purity more than 99.995%, nitrogen pressure is 0.4-0.5Mpa, and the temperature of degasification tank melt is 720-730 DEG C.
5. the anneal of aluminum foil for lithium battery according to claim 2, it is characterized in that, front case melt temperature 690-700 DEG C during continuous casting and rolling process, roll gap 4.6-4.8mm, roll 55-60mm, lip opening degree 11-12mm, preload force 180-260T, coiling tension: 40-60kn, roll casting speed 950-980mm/min, cooler-water temperature 32-38 DEG C.
6. the anneal of aluminum foil for lithium battery according to claim 1, it is characterized in that, aluminium foil finish rolling after second annealing process becomes after cold rolling thickness to be the aluminum foil coil of 0.01-0.05mm by aluminum foil for lithium battery blank, aluminum foil coil is cut to obtain finished product aluminum foil for lithium battery.
7. the anneal of aluminum foil for lithium battery according to claim 1, is characterized in that, during aluminum foil coil finish rolling process, F strain is 35-50N/mm
2, backward pull is 35-40N/mm
2, roll speed is 500-700m/min, and rolling load is 250-350T, and oil temperature is 50-55 DEG C, and oil pressure is 3.0-4.0bar, and flow is 50-65%, and roll crown is 0.06mm, gloss level of roll Ra0.12-0.2 μm, and rolling oil additives is 6-8%.
8. the anneal of aluminum foil for lithium battery according to claim 1, is characterized in that, composition and the mass percent thereof of described aluminum foil for lithium battery blank are: Fe:0.38-0.45%; Si:0.1-0.15%; Cu:0.03-0.06%; Ti:0.015-0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
9. the anneal of the aluminum foil for lithium battery according to claim 1 or 8, is characterized in that, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.38-0.42%; Si:0.12-0.15%; Cu:0.04-0.06%; Ti:0.018-0.02%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity.
10. the anneal of aluminum foil for lithium battery according to claim 9, is characterized in that, the composition of described aluminum foil for lithium battery and mass percent thereof are: Fe:0.39%; Si:0.12%; Cu:0.04%; Ti:0.016%; Mn :≤0.03%; Mg :≤0.03%; Zn :≤0.03%; Surplus is Al and inevitable impurity, wherein, and Mn+Mg+Zn≤0.03%.
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